TWI723425B - Method for producing eutectic layer of graphene and metal, electrically conductive wires and substrates - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 28
- 239000002184 metal Substances 0.000 title claims abstract description 28
- 239000000758 substrate Substances 0.000 title claims abstract description 21
- 230000005496 eutectics Effects 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 19
- 239000003792 electrolyte Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- FHMDYDAXYDRBGZ-UHFFFAOYSA-N platinum tin Chemical compound [Sn].[Pt] FHMDYDAXYDRBGZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 238000004534 enameling Methods 0.000 claims description 2
- 230000035699 permeability Effects 0.000 claims description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 15
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
Description
本發明係關於一種石墨烯與金屬形成共晶層之方法，尤指利用電解方式將石墨烯鍍在板材或導電線材上。 The present invention relates to a method for forming a eutectic layer between graphene and metal, in particular to electrolytically plating graphene on a plate or conductive wire.
石墨烯目前是世界上最薄且最堅硬的奈米材料，它幾乎是完全透明的，只吸收2~3%的光，然而因為導熱細數高達5300W/m*k，高於奈米管和金剛石，常溫下其電子遷移率超過15000cm2/V*s，又比奈米碳管或矽晶體(monocrystalline silicon)高，而電阻率只約10-6Ω*cm，比銅或銀更低，為目前世上電阻率最小的材料。 Graphene is currently the thinnest and hardest nanomaterial in the world. It is almost completely transparent and only absorbs 2~3% of light. However, because the thermal conductivity is as high as 5300W/m*k, it is higher than that of nanotubes and nanotubes. Diamond has an electron mobility of more than 15000 cm 2 /V*s at room temperature, which is higher than carbon nanotubes or monocrystalline silicon, and its resistivity is only about 10 -6 Ω*cm, which is lower than copper or silver. The material with the smallest resistivity in the world.
因為它的電阻率極低，電子的移動速度極快，因此被期待可用來發展出更薄、導電速度更快的新一代電子元件或電晶體。由於石墨烯實質上是一種透明、良好的導體，也適合用來製造透明觸控螢幕、光板、甚至是太陽能電池。 Because of its extremely low resistivity and extremely fast movement of electrons, it is expected to be used to develop a new generation of thinner and faster conducting electronic components or transistors. Since graphene is essentially a transparent and good conductor, it is also suitable for manufacturing transparent touch screens, light panels, and even solar cells.
但目前石墨烯在被使用在基材上時，常因傳統製程的缺失導致導電性不佳等問題發生，以下簡單描述： However, when graphene is currently used on a substrate, problems such as poor conductivity often occur due to the lack of traditional manufacturing processes. The following is a brief description:
傳統真空高頻濺/射鍍，使用此方式石墨烯層平均厚度約在20-30微米，所需的時間較長，雖然可以得到純度高的石墨烯層，但膜厚太薄，如果需要達到適合厚度(1-3層)，又因為石墨烯塗佈不易，難以多層堆疊，導致其物理性質(導電性、電磁性)效果不佳。又或者，這個方式要達到良好的電性及物性，必須多股載體線合一股，才能展現適當的電性及物性，這樣一來成本就相當高。 In traditional vacuum high-frequency sputtering/jet plating, the average thickness of the graphene layer in this method is about 20-30 microns, and it takes a long time. Although a high-purity graphene layer can be obtained, the film thickness is too thin. Suitable thickness (1-3 layers), and because graphene is not easy to coat, it is difficult to stack multiple layers, resulting in poor physical properties (conductivity, electromagnetic properties). Or, in order to achieve good electrical and physical properties in this way, multiple carrier wires must be combined to show proper electrical and physical properties, so the cost is quite high.
傳統填加法，高分子樹脂中添加石墨烯，但此方式因為樹脂的添加導致分散性不足，且介電係數太高，雖然膜厚夠，但仍無法表現出最佳的導電性、電磁性。 In the traditional filling method, graphene is added to the polymer resin, but this method has insufficient dispersibility due to the addition of the resin, and the dielectric coefficient is too high. Although the film thickness is sufficient, it still fails to exhibit the best electrical conductivity and electromagnetic properties.
為了解決上述傳統製程所導致的缺失，爰此，本發明人石墨烯塗佈方法，包含以下步驟：將一基材浸泡於一電解液中，所述電解液可為一硫酸銅溶液或一硫化鎳溶液，其中該電解液放入重量百分比0.5-3之一石墨烯，進行反應，使該基材外包覆厚度介於2到4微米之一石墨烯層，該石墨烯層含有一導電金屬層，再噴塗一金屬層至該基材上，使該石墨烯層包覆該金屬層，所包覆的該金屬層厚度介於2到5微米，再透過一導磁程序，將一氧化非晶體導磁層包覆前述石墨烯層，並透過一包覆程序，將一錫鉑薄膜包覆前述該氧化非晶體導磁層。 In order to solve the shortcomings caused by the above-mentioned traditional manufacturing process, the present inventors' graphene coating method includes the following steps: immersing a substrate in an electrolyte, the electrolyte may be a copper sulfate solution or a sulfurization solution. Nickel solution, where 0.5-3 weight percent of graphene is placed in the electrolyte to react, so that the substrate is coated with a graphene layer with a thickness of 2 to 4 microns, and the graphene layer contains a conductive metal Layer, and then spray a metal layer on the substrate so that the graphene layer covers the metal layer. The thickness of the metal layer covered is between 2 to 5 microns. The crystalline magnetic layer covers the graphene layer, and a tin-platinum film is coated on the oxidized amorphous magnetic layer through a coating process.
進一步，所述基材為一導電線材。進一步更包含有一漆包程序，用以將一樹脂包覆前述基材及前述石墨烯層。 Further, the substrate is a conductive wire. It further includes an enameling process for coating the substrate and the graphene layer with a resin.
進一步，所述基材可以是一板材。 Further, the substrate may be a plate.
本發明揭露一種導電線材，透過上述方式，將石墨烯塗佈在該導電線材表面。 The present invention discloses a conductive wire, through which graphene is coated on the surface of the conductive wire through the above-mentioned method.
本發明揭露一種板材，透過上述方式，將石墨烯塗佈在該板材表面。 The present invention discloses a sheet material, through which graphene is coated on the surface of the sheet material through the above-mentioned method.
根據上述技術特徵可達成以下功效： According to the above technical features, the following effects can be achieved:
1.本發明能夠製造出厚薄適中的石墨烯層，厚度約在於2到4微米，能提供最佳的導電性及導磁性。 1. The present invention can produce a graphene layer of moderate thickness with a thickness of about 2 to 4 microns, which can provide the best conductivity and magnetic permeability.
2.本發明製成時間短，相較於真空濺鍍製程所耗費的時間來比節省相當多。 2. The manufacturing time of the present invention is short, which saves a lot of time compared with the time consumed by the vacuum sputtering process.
1:銅線 1: Copper wire
2:石墨烯層 2: Graphene layer
21:導電金屬層 21: Conductive metal layer
22:銅層 22: Copper layer
3:樹脂外皮 3: Resin skin
4:氧化非晶體導磁層 4: Oxidized amorphous magnetic permeable layer
5:錫鉑薄膜 5: Tin platinum film
[第一圖]係本發明實施例之電解示意圖。 [The first figure] is a schematic diagram of electrolysis of an embodiment of the present invention.
[第二圖]係本發明實施例之流程示意圖。 [The second figure] is a schematic flow diagram of an embodiment of the present invention.
[第三圖]係本發明實施例之線材表面結構示意圖(一)。 [Third Figure] is a schematic diagram (1) of the wire surface structure of the embodiment of the present invention.
[第四圖]係本發明實施例之線材表面結構示意圖(二)。 [Fourth Figure] is a schematic diagram (2) of the surface structure of the wire according to the embodiment of the present invention.
[第五圖]係本發明實施例之線材剖面示意圖。 [Fifth Figure] is a schematic cross-sectional view of a wire rod according to an embodiment of the present invention.
[第六圖]係本發明實施例之SEM示意圖。 [Figure 6] is a schematic diagram of an SEM of an embodiment of the present invention.
綜合上述技術特徵，本發明石墨烯與金屬形成共晶層之方法的主要功效將可於下述實施例清楚呈現。 Based on the above technical features, the main effects of the method for forming a eutectic layer between graphene and metal of the present invention will be clearly demonstrated in the following embodiments.
請先參閱第一圖及第二圖所示，此圖示說明本發明之實施例，主要說明到石墨烯與金屬形成共晶層之方法，包含以下步驟： Please refer to the first and second diagrams. This diagram illustrates an embodiment of the present invention. It mainly describes the method for forming a eutectic layer between graphene and metal, which includes the following steps:
取一基材，所述基材在本實施例中為一導電線材，但不能做為限制條件，該基材也可以是板材，該板材可以為任意形狀。在第一實施例中我們所呈現的為電線的製程，主要是希望能在電線上塗佈適當厚度的石墨烯。首先，我們所取得的該基材為一銅線(1)，也可以為其他導電金屬，例如鋁、鐵等等導電金屬，先執行前處理清洗，可用化學清洗方式或是電漿清除表面髒汙，再將該銅線浸泡在一電解液中，所述電解液可為一硫酸銅溶液或一硫化鎳溶液，其中該電解液放入重量百分比0.5-3之一石墨烯(2)，進行反應，使該基材包覆厚度介於2到4微米之一石墨烯層，但此時的該石墨烯層(2)由於分布的情況非常不平均(顆粒狀態)，如第三圖所示，僅有在該石墨烯層(2)含有一導電金屬層(21)，該導電金屬層(21)在本實施例中採用一銅層(22)(但不依此為任何限制條件，可替換成一錫層或一鋅層等)，但顆粒狀態的該石墨烯層表面仍有斷開或是不相連的情況，易影響傳輸電的效率。 Take a substrate. The substrate is a conductive wire in this embodiment, but it cannot be used as a limiting condition. The substrate can also be a plate, and the plate can have any shape. In the first embodiment, what we presented is the manufacturing process of the wire, and it is mainly hoped that the appropriate thickness of graphene can be coated on the wire. First of all, the substrate we obtained is a copper wire (1), it can also be other conductive metals, such as aluminum, iron and other conductive metals. The pre-treatment cleaning is performed first. Chemical cleaning or plasma can be used to clean the surface. Dirty, and then soak the copper wire in an electrolyte, the electrolyte can be a copper sulfate solution or a nickel sulfide solution, wherein the electrolyte is put into 0.5-3 weight percent graphene (2), proceed The reaction causes the substrate to coat a graphene layer with a thickness of 2 to 4 microns, but the graphene layer (2) at this time is very uneven (particle state) due to the distribution, as shown in the third figure , Only the graphene layer (2) contains a conductive metal layer (21), and the conductive metal layer (21) uses a copper layer (22) in this embodiment (but it is not subject to any restriction and can be replaced It is a tin layer or a zinc layer, etc.), but the surface of the graphene layer in the granular state is still disconnected or disconnected, which easily affects the efficiency of power transmission.
請參考第四圖，為了避免上述提到的問題，進一步再噴塗一金屬層，在本實施例中該金屬層採用一銅層(22)(但不依此為任何限制條件，可替換成一錫層或一鋅層等)，至該基材上，使該石墨烯層(2)包覆該銅層(22)，所包覆的該銅層(22)厚度介於2到5微米，由於該銅層(22)為奈米大小，會均勻的包覆住該石墨烯層(2)，使得該石墨烯層(2)不會發生斷開的現象。補充說明銅的電阻約在(20℃)1.678×10-8Ω．m。 Please refer to the fourth figure, in order to avoid the above-mentioned problem, a metal layer is further sprayed. In this embodiment, the metal layer is a copper layer (22) (but it is not subject to any restrictions, and can be replaced with a tin layer. Or a zinc layer, etc.) on the substrate, so that the graphene layer (2) covers the copper layer (22), and the thickness of the covered copper layer (22) is between 2 to 5 microns. The copper layer (22) is nanometer-sized and will evenly cover the graphene layer (2), so that the graphene layer (2) will not be disconnected. It is added that the resistance of copper is about (20℃) 1.678×10-8Ω. m.
如第二圖所示，緊接著在對該銅線進行烘乾作業，可以是自然烘乾，或是施以溫度約40-60度，使表面完全乾燥，再包覆有一氧化非晶體導磁層(4)及一錫鉑薄膜(5)，其中氧化非晶體導磁層(4)可為鐵、鈷、鋯、鉀等金屬，主要是磁屏蔽材料，該些材料具有奈米級粉體混入一樹脂外皮(3)內，可以用以 避免電磁干擾。以及，該錫鉑薄膜(5)主要目的在於避免日後電線通電後，因電磁感應效應所產生的電磁波對周邊電子設備所造成的干擾影響。 As shown in the second figure, the copper wire is then dried. It can be dried naturally, or applied to a temperature of about 40-60 degrees to completely dry the surface, and then coated with amorphous oxide magnetism. Layer (4) and a tin-platinum film (5), wherein the oxidized amorphous magnetic layer (4) can be iron, cobalt, zirconium, potassium and other metals, mainly magnetic shielding materials, these materials have nano-level powder Mixed into a resin skin (3), can be used Avoid electromagnetic interference. And, the main purpose of the tin-platinum film (5) is to avoid interference effects on peripheral electronic devices caused by electromagnetic waves generated by electromagnetic induction effects after the wires are energized.
如第第五圖所示，我們可以清楚檢視到線材的剖面圖，可以了解其中的結構樣態，最內部為該銅線(1)，在該銅線(1)外包覆了塗佈完成的該石墨烯層(2)，最外層則是絕緣的該樹脂外皮(3)。同時也可以參閱第六圖所示，為SEM拍攝畫面，我們可以檢視到該石墨烯層(2)的厚度約在4微米上下。 As shown in the fifth figure, we can clearly view the cross-sectional view of the wire and understand the structure. The innermost part is the copper wire (1), and the copper wire (1) is covered with a coating. The graphene layer (2), the outermost layer is the insulating resin skin (3). At the same time, you can also refer to the sixth figure, which is a SEM shot. We can see that the thickness of the graphene layer (2) is about 4 microns.
本發明另揭露一種板材，使用如上述第一實施例中描述之石墨烯塗佈方法，將該板材表面塗佈有所述石墨烯層。 The present invention also discloses a sheet material, which is coated with the graphene layer on the surface of the sheet material using the graphene coating method described in the first embodiment above.
綜合上述實施例之說明，當可充分瞭解本發明之操作、使用及本發明產生之功效，惟以上所述實施例僅係為本發明之較佳實施例，當不能以此限定本發明實施之範圍，即依本發明申請專利範圍及發明說明內容所作簡單的等效變化與修飾，皆屬本發明涵蓋之範圍內。 Based on the description of the above embodiments, when one can fully understand the operation and use of the present invention and the effects of the present invention, but the above embodiments are only the preferred embodiments of the present invention, and the implementation of the present invention cannot be limited by this. The scope, that is, simple equivalent changes and modifications made according to the scope of the patent application of the present invention and the content of the description of the invention, are all within the scope of the present invention.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103943281A (en) * | 2014-05-09 | 2014-07-23 | 浙江大学 | Preparation method of electric wire and cable with copper-graphene complex phase conductive wire core |
| JP2016018714A (en) * | 2014-07-09 | 2016-02-01 | 株式会社クラレ | Conductive film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103943281A (en) * | 2014-05-09 | 2014-07-23 | 浙江大学 | Preparation method of electric wire and cable with copper-graphene complex phase conductive wire core |
| JP2016018714A (en) * | 2014-07-09 | 2016-02-01 | 株式会社クラレ | Conductive film |
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| TW202045602A (en) | 2020-12-16 |
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